CN103592274B - A kind of method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals - Google Patents
A kind of method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals Download PDFInfo
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- CN103592274B CN103592274B CN201310579034.6A CN201310579034A CN103592274B CN 103592274 B CN103592274 B CN 103592274B CN 201310579034 A CN201310579034 A CN 201310579034A CN 103592274 B CN103592274 B CN 103592274B
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- biphenthrin
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- OMFRMAHOUUJSGP-IRHGGOMRSA-N bifenthrin Chemical compound C1=CC=C(C=2C=CC=CC=2)C(C)=C1COC(=O)[C@@H]1[C@H](\C=C(/Cl)C(F)(F)F)C1(C)C OMFRMAHOUUJSGP-IRHGGOMRSA-N 0.000 title claims abstract description 52
- 239000000523 sample Substances 0.000 title claims abstract description 51
- 239000002096 quantum dot Substances 0.000 title claims abstract description 48
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000003905 agrochemical Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000000575 pesticide Substances 0.000 claims abstract description 24
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims abstract description 8
- VQXSOUPNOZTNAI-UHFFFAOYSA-N Pyrethrin I Natural products CC(=CC1CC1C(=O)OC2CC(=O)C(=C2C)CC=C/C=C)C VQXSOUPNOZTNAI-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000010290 biphenyl Nutrition 0.000 claims abstract description 4
- 239000004305 biphenyl Substances 0.000 claims abstract description 4
- 238000001514 detection method Methods 0.000 claims abstract description 4
- HYJYGLGUBUDSLJ-UHFFFAOYSA-N pyrethrin Natural products CCC(=O)OC1CC(=C)C2CC3OC3(C)C2C2OC(=O)C(=C)C12 HYJYGLGUBUDSLJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- VJFUPGQZSXIULQ-XIGJTORUSA-N pyrethrin II Chemical compound CC1(C)[C@H](/C=C(\C)C(=O)OC)[C@H]1C(=O)O[C@@H]1C(C)=C(C\C=C/C=C)C(=O)C1 VJFUPGQZSXIULQ-XIGJTORUSA-N 0.000 claims abstract description 4
- 238000010791 quenching Methods 0.000 claims abstract description 4
- 239000002159 nanocrystal Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 229910052793 cadmium Inorganic materials 0.000 claims description 6
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 6
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 claims description 6
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052711 selenium Inorganic materials 0.000 claims description 6
- 239000011669 selenium Substances 0.000 claims description 6
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- LAWOZCWGWDVVSG-UHFFFAOYSA-N dioctylamine Chemical compound CCCCCCCCNCCCCCCCC LAWOZCWGWDVVSG-UHFFFAOYSA-N 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 claims description 3
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 claims description 3
- 238000011896 sensitive detection Methods 0.000 abstract description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 241000238631 Hexapoda Species 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- MURGITYSBWUQTI-UHFFFAOYSA-N fluorescin Chemical compound OC(=O)C1=CC=CC=C1C1C2=CC=C(O)C=C2OC2=CC(O)=CC=C21 MURGITYSBWUQTI-UHFFFAOYSA-N 0.000 description 2
- 230000000749 insecticidal effect Effects 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000256844 Apis mellifera Species 0.000 description 1
- 241000255789 Bombyx mori Species 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
- 238000012742 biochemical analysis Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 230000003053 immunization Effects 0.000 description 1
- 238000002649 immunization Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000002728 pyrethroid Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
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Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals, can the fluorescence of effective quench fluorescence nanocrystal CdSe quantum dot probe based on Biphenthrin, therefore can utilize the Biphenthrin agricultural chemicals in Fluorescence-quenching rapid sensitive detection solution, can 5.1 × 10 be reached to the detectability of biphenyl pyrethrin pesticide
– 8mol/L, related coefficient is 0.9999.The inventive method is not only simple to operation, and highly sensitive, selectivity good, can realize the detection of the highly sensitive and high selectivity of Biphenthrin in biased sample.
Description
Technical field
The invention belongs to Biphenthrin Pesticides Testing technical field, be specifically related to a kind of method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals.
Background technology
Biphenthrin belongs to a kind of pyrethroid insecticidal/acaricidal agent, and insecticidal activity is very high, is mainly and tags and stomach poison function, there is not stifling and systemic action.Biphenthrin is a kind of broad spectrum pesticide, medium to honeybee toxicity, higher to silkworm toxicity.Biphenthrin has the feature that effect is rapid, the lasting period is long when acting on insect, have good prevention effect to many insects and multiple tetranychid simultaneously, but very high to fish toxicity.Up to now, the main detection adopting chromatography and immunization to carry out Biphenthrin agricultural chemicals, but there is complex operation, shortcoming that cost is high in these two class methods.Therefore, set up easy and simple to handle, simple Biphenthrin Pesticides Testing method and become Developing trend.
In recent years, fluorescence nano CdSe quantum dot probe causes the extensive concern of researchers gradually.Compare traditional organic fluorescent dye and fluorescin, quantum dot has many superior spectral qualities, as exciting light spectrum width, emission spectrum is narrow and symmetrical, fluorescence quantum yield is high, fluorescent stability is strong, anti-light bleachability is strong, and these superior spectral qualities make fluorescence nano CdSe quantum dot probe be widely used in biochemical analysis field.But, up to now, adopt the report of fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals there is not yet.
For above problem, we have studied a kind of new method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals, the method is simple to operate, highly sensitive, selectivity is good, can be used for the highly sensitive detection of Biphenthrin in mixed solution.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
1. the preparation method of fluorescence nano CdSe quantum dot probe is as follows:
Taking 0.05g selenium powder joins in the flask that 0.28g tri-n-butyl phosphine and 1.4g dioctylamine are housed, and leaves standstill 14h, prepares selenium storing solution; Get 0.018g cadmium oxide and 0.15g stearic acid in there-necked flask, be heated to 168 DEG C under argon shield and cadmium oxide is fully dissolved, prepare cadmium storing solution; 1.34g trioctylphosphine and 1.4g cetylamine is added in the cadmium storing solution made; stir under argon shield and be heated to 308 DEG C; the selenium storing solution taken out is injected in reaction vessel; continue 288 DEG C of reactions 90 seconds; after making product be cooled to room temperature, i.e. obtained fluorescence nano CdSe quantum dot probe.
2. the method for the fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals utilizing step 1 to prepare:
During application fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals, fluorescence nano CdSe quantum dot probe solution after dilution 25 times is mixed with Biphenthrin the pesticide solution, and the mol ratio of fluorescence nano CdSe quantum dot probe solution and Biphenthrin the pesticide solution is controlled in the scope of 1: 0.71 ~ 18, now Biphenthrin can the fluorescence of effective quench fluorescence nanocrystal CdSe quantum dot probe, and in good linear relationship between the fluorescence intensity of fluorescence nano CdSe quantum dot probe and Biphenthrin pesticide concentration, therefore, fluorescence nano CdSe quantum dot probe can as the probe detecting Biphenthrin agricultural chemicals, and energy rapid sensitive detects the content of Biphenthrin agricultural chemicals in hexane solution, 5.1 × 10 are limited to the detection of biphenyl pyrethrin pesticide
– 8mol/L.
Advantage of the present invention:
1. fluorescence nano CdSe quantum dot fluorescence probe intensity provided by the invention is high, fluorescent stability is high, anti-light bleachability is strong.
2. adopt the fluorescence nano CdSe quantum dot probe prepared by the present invention to detect biphenyl pyrethrin pesticide, there is easy and simple to handle, highly sensitive, that selectivity is good advantage.
Accompanying drawing explanation
Fig. 1 be fluorescence nano CdSe quantum dot probe of the present invention in Biphenthrin Pesticides Testing process, after different Biphenthrin pesticide concentration and fluorescence nano CdSe quantum dot probe reaction, the fluorescence spectrum figure of excitation wavelength for obtaining during 388nm;
In figure, a ~ e is the different Biphenthrin pesticide concentrations added in embodiment, make the mol ratio of probe and Biphenthrin agricultural chemicals be 1: 0.71 ~ 18 fluorescence spectrum figure.
Embodiment
For a better understanding of the present invention, below in conjunction with specific embodiment the present invention done and further elaborate.Should be understood that following examples are preferred implementations more of the present invention, object is to set forth content of the present invention better, instead of produces any restriction to protection scope of the present invention.
Embodiment 1
The preparation of fluorescence nano CdSe quantum dot probe:
Taking 0.05g selenium powder joins in the flask that 0.28g tri-n-butyl phosphine and 1.4g dioctylamine are housed, and leaves standstill 14h, prepares selenium storing solution; Get 0.018g cadmium oxide and 0.15g stearic acid in there-necked flask, be heated to 168 DEG C under argon shield and cadmium oxide is fully dissolved, prepare cadmium storing solution; 1.34g trioctylphosphine and 1.4g cetylamine is added in the cadmium storing solution made; stir under argon shield and be heated to 308 DEG C; the selenium storing solution taken out is injected in reaction vessel; continue 288 DEG C of reactions 90 seconds; after making product be cooled to room temperature, i.e. obtained fluorescence nano CdSe quantum dot probe.
Embodiment 2
A kind of method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals:
Application fluorescence nano CdSe quantum dot detects in the process of Biphenthrin agricultural chemicals in Biphenthrin standard sample of pesticide, fluorescence nano CdSe quantum dot probe solution after dilution 25 times is mixed with Biphenthrin the pesticide solution, make the mol ratio of fluorescence nano CdSe quantum dot probe solution and Biphenthrin the pesticide solution be 1: 0.71, namely obtain fluorescence spectrum a in Fig. 1.
Embodiment 3
A kind of method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals:
All the other conditions are all identical with step 1, and only the mol ratio of fluorescence nano CdSe quantum dot probe solution and Biphenthrin the pesticide solution changes 1: 2.8 into, then obtain fluorescence spectrum b in Fig. 1.
Embodiment 4
A kind of method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals:
All the other conditions are all identical with step 1, and only the mol ratio of fluorescence nano CdSe quantum dot probe solution and Biphenthrin the pesticide solution changes 1: 5.6 into, then obtain fluorescence spectrum c in Fig. 1.
Embodiment 5
A kind of method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals:
All the other conditions are all identical with step 1, and only the mol ratio of fluorescence nano CdSe quantum dot probe solution and Biphenthrin the pesticide solution changes 1: 10 into, then obtain fluorescence spectrum d in Fig. 1.
Embodiment 6
A kind of method utilizing fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals:
All the other conditions are all identical with step 1, and only the mol ratio of fluorescence nano CdSe quantum dot probe solution and Biphenthrin the pesticide solution changes 1: 18 into, then obtain fluorescence spectrum e in Fig. 1.
Can learn that the fluorescence intensity of fluorescence nano CdSe quantum dot probe weakens with the increase of the concentration of Biphenthrin agricultural chemicals from above embodiment fluorescence spectrum Fig. 1, and have good linear relationship between the decreasing value of fluorescence intensity and Biphenthrin pesticide concentration, R
2=0.9999.
Claims (1)
1. utilize a method for fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals, it is characterized in that,
1) preparation of fluorescence nano CdSe quantum dot probe:
Taking 0.05g selenium powder joins in the flask that 0.28g tri-n-butyl phosphine and 1.4g dioctylamine are housed, and leaves standstill 14h, prepares selenium storing solution; Get 0.018g cadmium oxide and 0.15g stearic acid in there-necked flask, be heated to 168 DEG C under argon shield and cadmium oxide is fully dissolved, prepare cadmium storing solution; 1.34g trioctylphosphine and 1.4g cetylamine is added in the cadmium storing solution made, stir under argon shield and be heated to 308 DEG C, the selenium storing solution taken out is injected in reaction vessel, continue 288 DEG C of reactions 90 seconds, after making product be cooled to room temperature, i.e. obtained fluorescence nano CdSe quantum dot probe;
2) step 1 is utilized) method of fluorescence nano CdSe quantum dot probe in detecting Biphenthrin agricultural chemicals prepared:
Fluorescence nano CdSe quantum dot probe solution after dilution 25 times is mixed with Biphenthrin the pesticide solution, and the mol ratio of fluorescence nano CdSe quantum dot probe solution and Biphenthrin the pesticide solution is controlled in the scope of 1: 0.71 ~ 18, now Biphenthrin can the fluorescence of effective quench fluorescence nanocrystal CdSe quantum dot probe, and in good linear relationship between the fluorescence intensity of fluorescence nano CdSe quantum dot probe and Biphenthrin pesticide concentration, therefore, fluorescence nano CdSe quantum dot probe can as the probe detecting Biphenthrin agricultural chemicals, and energy rapid sensitive detects the content of Biphenthrin agricultural chemicals in hexane solution, 5.1 × 10 are limited to the detection of biphenyl pyrethrin pesticide
– 8mol/L.
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Patent Citations (5)
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|---|---|---|---|---|
| WO2001061348A1 (en) * | 2000-02-16 | 2001-08-23 | Quantum Dot Corporation | Single target counting assays using semiconductor nanocrystals |
| WO2006081441A1 (en) * | 2005-01-28 | 2006-08-03 | Geosafe Corporation | Waste treatment by in-container vitrification |
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